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Salt Analysis

The document outlines a systematic approach to analyze inorganic salts for one acidic and one basic radical, detailing the necessary apparatus, theoretical background, and step-by-step procedures for qualitative analysis. It includes classifications of acidic and basic radicals, common ion effects, solubility products, and specific tests for identifying various ions. The document also emphasizes the importance of proper documentation and presentation of results in a practical file.
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0% found this document useful (0 votes)
34 views9 pages

Salt Analysis

The document outlines a systematic approach to analyze inorganic salts for one acidic and one basic radical, detailing the necessary apparatus, theoretical background, and step-by-step procedures for qualitative analysis. It includes classifications of acidic and basic radicals, common ion effects, solubility products, and specific tests for identifying various ions. The document also emphasizes the importance of proper documentation and presentation of results in a practical file.
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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SALT ANALYSIS

AIM: To analyse the given salt for one acidic and one basic radical systematically.

APPARATUS REQUIRED: Watch glass, test tubes, test tube holder, Bunsen burner, test tube cleaner, wash
bottle etc.

THEORY:

 Qualitative analysis of inorganic salts means the identification of cations and anions present in the
salt or a mixture of salts.
 In the formation of a salt, the part contributed by the acid is called anion or acid radical and the part
contributed by the base is called cation or basic radical.

For example, in the salts CuSO4 and NaCl, Cu2+ and Na+ ions are cations or basic radical and
SO42– and Cl– ions are anions or acid radical.

 Systematic analysis of an inorganic salt involves the following steps:

(i) Preliminary examination of solid salt and its solution.

(ii) Determination of anions by reactions carried out in solution (wet tests) and confirmatory tests.

(iii) Determination of cations by reactions carried out in solution (wet tests) and confirmatory tests.

 Classification of Acidic Radical:

(1) Dilute Sulphuric Acid Group: CO32-, SO32-, S2-, NO2-

(2) Concentrated Sulphuric Acid Group: Cl-, Br-, I-, CH3COO-, C2O42-, and NO3-

(3) Independent Group – SO42-, PO43-

 Classification of Basic Radical:

Group Cation Group Reagent Form of Precipitation


Group Zero NH4+ None -
Group I Pb2+ Dilute HCl Chloride
Group II Pb2+, Cu2+, As3+ H2S gas in presence of dil. HCl Sulphides
Group III Al3+, Fe3+ NH4OH in presence of NH4Cl Hydroxides
Group IV Co2+, Ni2+, Mn2+, Zn2+ H2S gas in presence of NH4OH Sulphides
Group V Ba2+, Sr2+, Ca2+ (NH4)2CO3 in presence of NH4OH Carbonates
Group VI Mg2+ None -

 Common Ion Effect: The common-ion effect refers to the decrease in solubility of an ionic
precipitate by the addition to the solution of a soluble compound with an ion in common with the
precipitate.

For example:
Hydrogen sulphide (H2S) is a weak electrolyte. It is partially ionized when in aqueous solution,
therefore there exists an equilibrium between un-ionized molecules and constituent ions in an
aqueous medium as follows:

H2S ⇌ H+ + HS−

Hydrochloric acid (HCl) is a strong electrolyte, which nearly completely ionizes as

HCl → H+ + Cl−

If HCl is added to the H2S solution, H+ a common ion and creates a common ion effect. Due to
+
the increase in concentration of H ions from the added HCl, the equilibrium of the dissociation of H2S
shifts to the left and keeps the value of Ka constant. Thus the dissociation of H2S decreases, the
concentration of un-ionized H2S increases, and as a result, the concentration of sulphide ions decreases.

 Solubility Product: The solubility product constant is the equilibrium constant for the dissolution of a
solid substance into an aqueous solution. It is denoted by the symbol Ksp.

Its value depends on temperature. Ksp usually increases with an increase in temperature due
to increased solubility.

 Ionic Product: It is the product of the concentrations of the ions in solution raised to the same
powers as in the solubility product expression.
 Condition for precipitation: When Ionic product is greater than solubility product, then precipitation
occurs.

PHYSICAL EXAMINATION OF THE SALT:

1) State:
2) Colour:
3) Odour:
4) Solubility in Water:

TESTS FOR ACID RADICALS:

Experiment Observation Inference


1. Dilute Sulphuric Acid Group

TESTS FOR BASIC RADICALS:

Experiment Observation Inference


1. Zero Group

RESULT: The given salt was found to contain ____ as acidic radical and ______ as basic radical.

PRECAUTIONS: Any 2
SCHEME OF ANALYSIS:

ACID RADICALS

Experiment Observation Inference


1. Dilute Sulphuric Acid Colorless, odourless gas with brisk effervescence, which Carbonate, CO32-
Group turns lime water milky may be present
To a small amount of salt in a
clean test tube, 2-3 mL of Colorless gas with rotten egg smell Sulphide, S2- may
Dilute H2SO4 was added be present

Colorless gas with pungent smell Sulphite, SO32-


may be present

Brown fumes Nitrite, NO2- may


be present

 If any of the above observation is seen, proceed for the confirmatory test of that ion.
 If none of the above observations are seen move to concentrated sulphuric acid group.

2. Concentrated Sulphuric A colourless gas with pungent smell, which gives dense Chloride, Cl- may
Acid Group white fumes when a rod dipped in ammonium hydroxide is be present
To a small amount of salt brought near the mouth of the test tube.
in a clean and dry test
tube, 2-3 drops of Con.
H2SO4 was added

Reddish brown gas with a pungent odour is evolved Bromide, Br- may
be present

Deep Violet vapours evolved Iodide, I- may be


present

Colourless, odourless gas is evolved which turns lime water Oxalate, C2O42-
milky may be present

Colourless vapours with smell of vinegar. Acetate,


CH3COO- may be
present

Cu turnings were added Brown fumes evolved Nitrate, NO3-


to the above test tube may be present
and test tube was heated
(when none of the five
observations are seen)

 If any of the above observation is seen, proceed for the confirmatory test of that ion.
 If none of the above observations are seen move to independent group.
3. Independent Group:
a) Sulphate:
To the aqueous solution
of salt, few drops of dil. white ppt insoluble in conc. HCl Sulphate, SO42-
HCl were added followed confirmed
by BaCl2 solution

b) Phosphate:
To the aqueous solution
of salt, few drops of conc. Canary yellow ppt
HNO3 were added
followed by ammonium Phosphate, PO43-
molybdate solution and confirmed
test tube was heated

Confirmatory tests
Chloride, Bromide and A curdy white precipitate soluble in ammonium hydroxide Chloride, Cl-
Iodide - Silver Nitrate confirmed
Test:
To the aqueous solution
of salt, few drops of
HNO3 solution and AgNO3
solutions were added A pale yellow precipitate which dissolves in ammonium Bromide, Br-
hydroxide with difficulty confirmed

Appearance of a yellow precipitate insoluble in excess Iodide, I-


of NH4OH confirmed

Acetate: formation of red ppt which becomes brown red on heating Acetate,
To the aqueos solution of CH3COO-
salt, neutral FeCl3 confirmed
solution was added

Nitrate:
To the aqueous solution
of the salt, freshly A brown ring formed at the junction of the two liquids Nitrate, NO3-
prepared aqueous confirmed
solution of FeSO4 was
added. Con. H2SO4 was
added from the sides of
the test tube, by keeping
the test tube at 45° angle.
BASIC RADICALS

Before proceeding with group tests, platinum wire test can be carried out as a cheat test. It is to be
reported only when a confirmed flame colour is obtained.

Experiment Observation Inference


Platinum Wire Test: Apple Green Flame Barium, Ba2+ may
A paste of salt in HCl solution be present
was prepared clean loop of Crimson red flame Strontium, Sr2+
Pt wire was dipped in the may be present
paste and it was heated in Brick red flame Calcium, Ca2+
oxidising flame. may be present

Experiment Observation Inference


1. Group Zero ( NH4+):
To the small amount of Ammoniacal smell Ammonium
salt in a clean test tube, ion, NH4+ may
NaOH solution was be present
added,and the test tube
was heated

Confirmatory test: Brown ppt (of basic mercury(II) amido-iodine) on cotton NH4+ confirmed
A cotton dipped in
Nessler’s reagent was
brought near the mouth
of test tube
 If ammoniacal smell is observed, proceed for the confirmatory test otherwise
move to group I
2. Group I ( Pb2+):
To the aqueous solution White ppt formed Pb2+ may be
of salt in a clean test Pb2+ + HCl → PbCl2 + 2H+ present
tube, 2-3 mL of dil. HCl white ppt
was added

Confirmatory test: Yellow ppt of lead iodide obtained


a) Potassium iodide, KI Pb2+ confirmed
solution was added to
the white ppt dissolved
in hot water
Yellow ppt of lead chromate obtained
b) Potassium chromate,
K2CrO4 solution was
added to the white ppt
dissolved in hot water
 If white ppt is observed, proceed for the confirmatory test otherwise
move to group II
2+
3. Group II ( Cu ):
Through the filtrate of Black ppt formed Cu2+ may be
2+ +
group I, H2S gas was Cu + H2S → CuS + 2H present (Note:
passed black ppt Colour of the
salt would be
Confirmatory test: blue)
The precipitate was A chocolate brown precipitate formed
boiled with dilute nitric Cu2+ Confirmed
acid and excess of
ammonium hydroxide
solution was added. A
blue solution
was obtained, which
was acidified with
acetic acid and
potassium ferrocyanide
solution was added
 If black ppt is observed with H2S gas, proceed for the confirmatory test otherwise
move to group III
3+ 3+
4. Group III ( Al , Fe ): Brown precipitate Fe3+ may be
H2S gas was boiled off present (Note:
from the filtrate of Colour of the
group II, 2-3 drops of salt would be
conc. HNO3 was added light green or
and test tube was brown)
heated. Then after
cooling a small amount A gelatinous white precipitate Al3+ may be
of solid ammonium present
chloride (NH4Cl) and an
excess of ammonium
hydroxide (NH4OH)
solution till it smells of
ammonia was added

Confirmatory test for


Fe3+:
A Prussian blue precipitate/colouration Fe3+ confirmed
The brown ppt was
dissolved in dil. HCl and
potassium ferrocyanide
solution was added

Confirmatory test for


Al3+: (BLue Lake Test)
Al3+ confirmed
The white ppt was Blue floating mass in the colourless solution
dissolved in dil. HCl and
blue litmus solution and
then ammonium
hydroxide solution drop
by drop along the sides
of the test tube was
added
 If brown/ white ppt is observed, proceed for the confirmatory test of the respective ion otherwise
move to group IV
5. Group IV ( Zn2+, Mn2+,
Co2+, Ni2+): Zn2+ may be
Through the filtrate of dirty white ppt present (Note:
group III, H2S gas was Zn2+ + H2S → ZnS + 2H+ Colour of the
passed white ppt salt would be
white)
buff coloured ppt ( skin coloured ppt) Mn2+ may be
Mn2+ + H2S → MnS + 2H+ present(Note:
buff ppt Colour of the
salt would be
light pink)
Black ppt Ni2+ or Co2+
Ni2+ + H2S → NiS + 2H+ may be present
black ppt (Note: Colour
Co2+ + H2S → CoS + 2H+ of the salt
black ppt would be dark
green if Ni2+
and magenta if
Co2+)
Confirmatory test for
Zn2+:
The precipitate was A bluish white precipitate Zn2+ confirmed
dissolved in dilute HCl
and ammonium
hydroxide solution
and potassium
ferrocyanide solutions
were added

Confirmatory test for


A white precipitate formed which turns brown on keeping.
Mn2+: Mn2+ confirmed
The precipitate was
dissolved in dilute HCl
and then sodium
hydroxide solution was
added in excess

Confirmatory test for


Ni2+:
The precipitate was a bright red precipitate Ni2+ confirmed
dissolved in aqua regia.
Ammonium hydroxide
solution was added till it
becomes alkaline and
then a few drops of
dimethyl glyoxime
solution was added

Confirmatory test for


Co2+:
The precipitate was A yellow precipitate Co2+ confirmed
dissolved in aqua regia.
Ammonium hydroxide
solution was added. The
solution was acidified
with dilute acetic acid
and solid potassium
nitrite was added
 If white/ buff/ black ppt is observed, proceed for the confirmatory test of the respective ion
otherwise move to group V
2+ 2+
6. Group V ( Ba , Sr ,
Ca2+): a white precipitate
H2S gas was boiled off Ba2+ + (NH4)2CO3 → BaCO3 + 2NH4+ Ba2+, Sr2+, Ca2+
from the filtrate of white ppt may be present
group IV and Sr2+ + (NH4)2CO3 → SrCO3 + 2NH4+
ammonium carbonate white ppt
solution was added Ca2+ + (NH4)2CO3 → CaCO3 + 2NH4+
white ppt

Confirmatory tests:
The ppt was dissolved in
acetic acid and the
solution was divided
into three parts

Confirmatory test for


Ba2+: Yellow precipitate Ba2+confirmed
a) To the first part,
potassium chromate
solution was added

b) Pt wire test Apple Green flame

Confirmatory test for


Sr2+: White precipitate Sr2+confirmed
a) To the second part,
ammonium sulphate
solution was added

b) Pt wire test Crimson-red flame

Confirmatory test for


Ca2+:
a) To the third part, White precipitate Ca2+confirmed
ammonium oxalate
solution was added

b) Pt wire test
Brick red flame
 If white ppt is observed with ammonium carbonate solution, proceed for the confirmatory test of
the ions otherwise move to group VI
2+
7. Group VI ( Mg ):
To the aqueous solution white crystalline precipitate Mg2+confirmed
of the salt, disodium
hydrogenphosphate
solution was added

NOTE:

 While writing the experiment in the practical file, everything has to be written on right side(ruled
side).
 Only write chemical equations of the confirmed ions on the ruled side (blank side), as given above
with the help of pencil only in front of the chemical test.
 Draw the tables for the experiment/observation and inference with the help of pencil and scale only.
Do not use pen.
 After finishing the acidic and basic radicals, write the result as: “The given salt was found to contain
____ as acidic radical and ______ as basic radical.”
 End your experiment with at least two precautions.
 DO not forget to write the date of the experiment on which you performed it and fill the index with
complete aim.

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